US20060251762A1 - Grain wet milling process for producing ethanol - Google Patents

Grain wet milling process for producing ethanol Download PDF

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US20060251762A1
US20060251762A1 US11/121,295 US12129505A US2006251762A1 US 20060251762 A1 US20060251762 A1 US 20060251762A1 US 12129505 A US12129505 A US 12129505A US 2006251762 A1 US2006251762 A1 US 2006251762A1
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protein
producing
temperature
grain
wheat
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Robert Jansen
John Kerr
Edward Farley
Gordon Walker
Sebastien Camborieux
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Primary Products Ingredients Americas LLC
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Assigned to TATE AND LYLE INGREDIENTS AMERICAS, INC. reassignment TATE AND LYLE INGREDIENTS AMERICAS, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CAMBORIEUX, SEBASTIEN, FARLEY, EDWARD, JANSEN, ROBERT, KERR, JOHN, WALKER, GORDON
Priority to EP06752023A priority patent/EP1880013A2/fr
Priority to AU2006242258A priority patent/AU2006242258A1/en
Priority to PCT/US2006/016661 priority patent/WO2006119206A2/fr
Publication of US20060251762A1 publication Critical patent/US20060251762A1/en
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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06—Ethanol, i.e. non-beverage
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • Wheat comprises starch, germ, bran, and a protein known as gluten. It is desirable to separate the constituents of wheat into separate materials. Wheat can be processed by dry milling wheat grains to remove the bran and the germ, then milling the remainder of the grains to produce wheat flour. The wheat flour can be further processed in order to generate separate starch, protein, and/or other products. Processing of the flour often involves separating starch from gluten. These process steps are typically done at a relatively low temperature, for example about 30° C. The starch can optionally be hydrolyzed and saccharified to produce dextrose, or can be fermented after or with saccharification to produce ethanol. Often a lower grade starch that is difficult to purify is used to make ethanol. The gluten produced in conventional wheat processes is vital wheat gluten, which has visco-elastic properties that are valuable in some situations.
  • Another problem with conventional wheat processes stems from the low temperatures used. At these temperatures, it is difficult to prevent the growth of microorganisms, which leads to unwanted fermentation, loss of yield and problems with product quality.
  • chemicals to control micro-organisms such as sodium hypochlorite and chlorine dioxide are added.
  • Caustic soda is often added to ensure that the pH does not drop too low due to the production of organic acids by the unwanted fermentation.
  • the use of these chemicals can affect the functional visco-elastic properties of the vital wheat gluten, reducing its quality.
  • An alternative to adding chemicals is to use more water rather than recycling, but this leads to extra energy costs to evaporate the water.
  • One aspect of the invention is a process that comprises (a) steeping at least one of wheat, barley, rye, or rice in an aqueous liquid to produce softened grain, (b) milling the softened grain to produce milled grain, (c) liquefying the milled grain by contacting it with amylase and heating it to a temperature of at least about 50° C., producing a liquefied material, (d) at least partially saccharifying the liquefied material by contacting it with amyloglucosidase at a temperature of at least about 50° C., producing a first saccharified material, and (e) separating fiber and germ from the first saccharified material, producing a screened material that is substantially free of fiber and germ.
  • the process also includes the steps of (f) further saccharifying and fermenting the screened material with a microorganism that produces ethanol, thereby producing a broth that comprises ethanol and insoluble protein, and (g) separating ethanol from the broth.
  • the insoluble protein which comprises both protein from the feed grain and microorganism from the fermenting, can also be separated as a protein-rich product.
  • the grain before steeping the wheat, barley, rye, and/or rice, the grain can be at least partially dehulled by milling. This removes at least some of the bran from the grain. The partially dehulled grain can then be steeped and further processed as described above.
  • compositions that are produced by the process described above.
  • the composition can comprise at least 60% by weight protein, and no more than about 1.5% by weight reducing sugars, both on a dry solids basis, and further contains no more than about 10% by weight moisture.
  • this composition is non-binding, and unlike corn gluten meal, it is not yellow.
  • the composition has a L* value of at least about 70, an a* value of no greater than about 5, and a b* value of no greater than about 20 on the Hunter color scale.
  • the composition has an a* value of no greater than about 3 and a b* value of no greater than about 15 on the Hunter color scale.
  • One embodiment of the process comprises a dextrose-producing line of steps and an ethanol-producing line of steps.
  • the dextrose-producing line of steps comprises:
  • (d-4) at least partially saccharifying the liquefied material by contacting it with amyloglucosidase at a temperature of at least about 50° C., producing a first saccharified material;
  • (d-6) further saccharifying the screened material by contacting it with amyloglucosidase at a temperature of at least about 50° C., producing a second saccharified material;
  • (e-4) at least partially saccharifying the liquefied material by contacting it with amyloglucosidase at a temperature of at least about 50° C., producing a first saccharified material;
  • step (e-5) combining the first fiber and germ stream from step (d-5) with the first saccharified material from step (e-4), and separating fiber and germ therefrom, producing a screened material that is substantially free of fiber and germ and a second fiber and germ stream;
  • the retentate from step (d-7) and the raffinate from step (d-8) can be added to the screened material from step (e-5) for fermenting in step (e-6).
  • FIG. 1 is a process flow diagram of an embodiment of the invention in which ethanol, gluten, and high-fiber animal feed products are produced from wheat.
  • FIG. 2 is a process flow diagram of another embodiment of the invention in which dextrose, protein, and ethanol products are recovered.
  • One embodiment of the invention is a process that can produce ethanol, a high protein product, and a high fiber product from wheat.
  • Other grains such as barley, rice, or rye can also be used, as well as combinations of two or more of these grains.
  • the feed grain can be at least partially dehulled by milling, for example in a Buhler mill or a Satake mill. This removes some of the bran in the feed grain, and tends to reduce the yield of starch and protein.
  • the process involves steeping wheat in an aqueous liquid to produce softened wheat.
  • the wheat grains can be steeped, for example, in water or an aqueous solution to which SO 2 has been added.
  • the softened wheat, or softened partially dehulled wheat is then milled.
  • the milled wheat is then liquefied by contacting it with amylase and heating it to a temperature of at least about 50° C., or in some cases, at least about 55° C. or at least about 70° C.
  • the liquefied material is at least partially saccharified by contacting it with amyloglucosidase at a temperature of at least about 50° C., or in some case at least about 55° C. or at least about 70° C.
  • This saccharification step results in a first saccharified material, which is then processed in a separation step.
  • the separation which can be performed, for example, by screening, separates fiber and wheat germ from the first saccharified material.
  • the separated fiber and wheat germ are suitable for use as animal feed.
  • the screened material that remains is substantially free of fiber and wheat germ (i.e., the combined concentration of fiber and germ in the screened material is no more than about 5% by weight, and in some embodiments is much less than 5%, for example 1% or less).
  • the screened material is fermented with a microorganism that produces ethanol, thereby producing a broth that comprises ethanol, soluble protein, and insoluble protein.
  • the ethanol can then be separated from the broth and recovered.
  • the process conditions can vary, in one embodiment of the process, the following conditions are used.
  • the aqueous liquid is maintained at a temperature of about 40-60° C. and pH of about 5-6 during steeping.
  • the milled wheat is maintained at a temperature of about 80-120° C. for about 0.5-5.0 hours during liquefying.
  • the liquefied material is cooled to about 55-65° C. prior to saccharifying, and the liquefied material is maintained at a temperature of about 55-68° C. and a pH of about 4-4.5 for about 2-15 hours during first saccharifying.
  • the fermentation is done at a temperature of about 20-35° C. and a pH of about 3.5-4.5.
  • SO 2 can be added to the aqueous liquid during steeping, and phospholipase and/or pentosanase can be used in the saccharifying step in addition to amyloglucosidase.
  • the process can further comprise separating the broth into an insoluble protein-rich stream and a liquid effluent stream.
  • a protein-rich product can be recovered from the insoluble protein-rich stream.
  • This protein-rich product comprises both protein (e.g., gluten) from the feed grain and microorganism (e.g., yeast) from the fermentation, and will be described further below.
  • the liquid effluent stream can be recycled to the milling step or elsewhere in the process.
  • the feed material for the process is whole grain wheat cereal 110 .
  • the wheat is cleaned of straw and stones, usually by screening.
  • the cleaned whole wheat is added to a steep tank 112 , where it is soaked in water 114 to soften the grain.
  • Sulfur dioxide 116 is also added to the steep tank.
  • the steeping system can be either batch or continuous and the residence time of the wheat is about 16 hours.
  • the temperature during the steep is 50° C.
  • the wheat is then separated from the steep water with a screen and a waste stream 120 can be withdrawn.
  • the steeped wheat is milled 122 , and this mill can be one or more of a variety of mills, but preferably is a toothed disc mill.
  • the pH of the milled wheat slurry is adjusted to 5.6 and alpha amylase enzyme 124 is added to liquefy the starch content of the stream.
  • the temperature is increased, for example to about 80-110° C., and the operation can be carried out in a starch cooker 126 .
  • the dry solids content of the liquefied material at this stage of the operation is about 15 to 20% d.s.
  • the material is held for about 5 minutes, for example in a length of pipe sized for the purpose, to allow the liquefaction time to proceed.
  • the slurry is then flashed to 98° C. and held for about 3 hours to allow liquefaction to complete.
  • the temperature of the liquefied material is then reduced to 62° C. and the pH adjusted to 4.2 and amyloglucosidase enzyme 128 is added. Phospholipase and pentosanase can be added at the same time. It is held for 2 to 12 hours to allow saccharification 130 to start and the viscosity to reduce.
  • This partially-saccharified slurry is then screened 132 to remove fiber and germ. This can be done in a number of stages, using water to wash the sugars from the fiber in a counter-current manner. This water can be added in the final fiber screen, with the wash water then progressing to the first screen. Suitable types of screens include DSM screens and centrifugal screens.
  • the washed fiber and germ 134 can be pressed, for example in a screw press 136 , and then dried 138 , milled, and sold as an animal feed 140 .
  • the screened material 142 from the fiber removal system 132 is placed in a fermenter 144 with a microorganism that can produce ethanol.
  • Suitable microorganisms for this purpose include Saccharomyces cerevisiae, Saccharomyces carlsbergiensis, Kluyveromyces lactis, Kluyveromyces fragilis, and any other microorganism that makes ethanol and is acceptable as an animal feed. This includes genetically modified yeasts that are acceptable as animal feed. Further saccharification can also take place in the fermenter as a result of the presence of amyloglucosidase.
  • the resulting fermentation broth 146 comprises wheat protein, yeast, and ethanol.
  • the ethanol 150 can be separated from the broth in a distillation unit 148 . Suitable distillation temperatures can be about 60-110° C. Optionally, it can then be subjected to rectification and dehydration, to produce a fuel-grade ethanol product. Another option is to produce potable ethanol by rectification.
  • the material 152 remaining from the fermentation broth after separation of the ethanol can then be further purified by membrane filtration, for example in an ultrafiltration unit 154 .
  • the permeate 156 from this membrane filtration can be disposed of as a waste stream or recycled in the process.
  • the retentate 158 from the membrane filtration which comprises insoluble protein, optionally with some water added, is dried in a drier 160 to yield a protein-rich product 162 .
  • This protein-rich product is a combination of the wheat protein that was present in the feed 110 and the yeast or other microorganism used in the fermentation.
  • the protein-rich product can be combined with the fiber-germ material 140 for use as an animal feed.
  • the protein-rich product 162 will typically have low reducing sugar content (e.g., less than about 1.5% by weight) and color similar to conventional dried vital wheat gluten.
  • the low content of reducing sugar makes the product easier to dry.
  • High dextrose content in a protein product could cause charring or even fire during drying of the product.
  • the yield of protein in some embodiments of the process, can be considerably higher than in a conventional wheat process, for example as much as 13 wt % or even higher, as compared to about 6% in a conventional process.
  • the gluten can be denatured by the heating in the process, the increased gluten yield can maintain the total value of the protein product as compared to that produced by a conventional wheat process.
  • the protein-rich product is a composition that comprises at least 60% by weight protein, no more than about 1.5% by weight reducing sugars (e.g., dextrose), and about 5% by weight moisture.
  • this composition is non-binding, and unlike corn gluten meal, it is not yellow.
  • the value of b* where a higher value represents a more yellow color, is relatively low.
  • the protein-rich product has a value typically less than half the value given by corn gluten meal, a value of b* of about 14 compared to 35.
  • FIG. 2 shows another version of the process in which a dextrose product is produced, in addition to ethanol and protein products.
  • Wheat 200 is cleaned by screening and added to two separate step tanks 202 and 204 , in which it is steeped as described above. The wheat is then separated from the steep water in each of the two tanks with a screen and is milled. Alpha amylase is added to the milled wheat from steep tank 202 to liquefy 206 the starch content of the material. Temperature and pH are adjusted as described above, and amyloglucosidase is added to saccharify the material. This partially-saccharified slurry 208 is screened to remove fiber and germ 210 .
  • the slurry that passes through the screens is then contacted with additional amyloglucosidase for further saccharification 212 .
  • the saccharified material produced by this operation is then membrane filtered 214 , for example by ultrafiltration, producing a permeate 216 and a retentate 218 .
  • the permeate 216 is purified by chromatographic separation 219 in a simulated moving bed unit, usually after pretreatment with carbon and/or softening, as described above.
  • the chromatographic separation 219 yields a dextrose-rich stream 220 and a second 222 stream comprising maltose, oligosaccharides, ash, and soluble protein.
  • the dextrose-rich stream 220 can be further refined 224 by carbon treatment and/or ion exchange, and then dried to produce a dextrose product 226 , such as a dextrose syrup.
  • the milled wheat from steep tank 204 can be liquefied 230 with alpha amylase and saccharified with amyloglucosidase.
  • the fiber and germ stream 210 from the screening step 208 can be combined with the partially saccharified slurry, which can then be screened 232 to separate the majority of the fiber and germ from the rest of the stream.
  • the fiber and germ can be recovered as a product stream 234 .
  • the resulting fermentation broth 238 comprises wheat protein, yeast, and ethanol.
  • the ethanol 240 can be separated from the broth in a distillation unit 242 . Optionally, it can then be subjected to rectification and dehydration, to produce a fuel-grade ethanol product. Another option is to produce potable ethanol by rectification.
  • the material 244 remaining from the fermentation broth after separation of the ethanol can then be further purified by membrane filtration 246 , for example in an ultrafiltration unit.
  • the permeate from this membrane filtration (not shown in FIG. 2 ) can be disposed of as a waste stream or recycled in the process.
  • the retentate 248 from the membrane filtration which comprises insoluble protein, optionally with some water added for diafiltration, is dried in a drier 250 to yield a protein-rich product 252 .
  • This protein-rich product is a combination of the wheat protein that was present in the feed 200 and the yeast or other microorganism used in the fermentation.
  • the protein-rich product can be combined with the fiber-germ material 234 for use as an animal feed.
  • the protein-rich product 252 will typically have the properties described above, such as low reducing sugar content (e.g., less than about 1.5% by weight), non-binding, and non-yellow color.
  • a batch of whole wheat weighing 200 kg (dry solids (DS) 88.8%, protein 11.6% and ash 1.4%) was prepared by screening to remove stones and other unwanted material.
  • This 200 kg of wheat was mixed with 550 liters of water in a 1 cu. meter tank. The mix was heated and kept at a temperature of 50° C. and sulphur dioxide was added as a 6% weight solution to a total of 1000 ppm.
  • the pH of the mix was pH 6.1 and it was held for 18 hours.
  • the temperature of the liquefied mixture was reduced to 62° C., and the pH was reduced to pH 4.2 with dilute hydrochloric acid.
  • Three enzymes were then added to the mix. These were 165 g of an amyloglucosidase enzyme, Dextrozyme DX, 155 g of a pentosanase enzyme, Shearzyme Plus, and 24 g of a phospholipase enzyme, Finizym W. All of these enzymes were supplied by Novozyme. The batch was then held for 4 hours to allow these enzymes to act.
  • the complete batch of material was then screened using a Sweco vibrating screen with a 100 micron mesh, the screening time being about 2 hours. This screening removed fiber from the slurry.
  • the first batch of slurry produced by screening (Batch 1), with a volume of 600 liters was put into a 1 cubic meter fermentation tank. It was cooled to 30° C. and water was added to reduce the dry solids from 13% down to 9%, giving a total of about 900 liters.
  • the fermentation was carried out by adding 225 g of Superstart yeast slurried in 1 liter of water. This yeast was Saccharomyces cerevisiae. Also added were 391 g of a 40% solution of urea as a nitrogen source.
  • the slurry was then ultrafiltered on a ceramic ultrafilter having 2 square meters of membrane with a 0.05 micron pore size. This material was ultrafiltered until the retentate volume was 50 liters. Diafiltration was not carried out and the analysis of the permeate and the retentate are given in Table 1.
  • Tests were carried out to dry the filtered slurry on two different types of drier, a spray drier and a ring drier. These two driers were the same driers as tested to dry batch 1 and their descriptions are above.
  • the spray drying test used an atomizing pressure of 5 Barg.
  • the inlet air temperature was 230° C. and the outlet temperature was 93° C.
  • the dried material collected had 3.5% moisture and the bulk of the material was collected in the product container, with little material sticking to the walls of the drier.
  • the ring drier was tested by mixing some of the previously spray dried material with slurry to get a moisture content of 35.7% This moisture was judged to give a material that could be fed to the ring drier.
  • the inlet air temperature of the drier was 250° C. and the outlet temperature was 95° C. The temperatures and the air flow to the drier were very steady and the product was collected from the product container. Its moisture content was 4.0% and analysis was as in Table 1.
  • the retentate was then diafiltered twice to remove dextrose. For the first diafiltration 50 liters of water was added and 50 liters of permeate were collected. This was repeated with the addition of 40 liters of water and the collection of 40 liters of permeate.
  • the resulting diafiltered retentate slurry contained protein and its analysis is shown in Table 2. Approximately 55 liters of this were collected and refrigerated prior to drying.
  • Two different driers were tested for this material. These were a spray drier and a ring drier.
  • the drier was opened and the dried material was found to be stuck to the walls and ceiling of the drier chamber. This was scraped off and a total of 1.16 kg collected with a moisture content of 12.4%. Some of this material had charred, particularly the material stuck to the ceiling of the drying chamber.
  • the second drier used was a pilot ring drier with a 3 inch ring with a classifier and a disintegrator.
  • This type of drier cannot be fed with a slurry and in order to feed it some of the slurry was mixed with some of the dried powder produced by the spray drier. Portions of these were mixed together to give a feed material with a moisture content of 26.4%, which was judged to be a mixture suitable for feeding to the ring drier.
  • This material was fed to the ring drier using an air inlet temperature of 250° C. The feed rate was maintained in an attempt to keep an outlet temperature of 95° C. The unit was unstable with the inlet air temperature changing, indicating that the air flow was not stable.
  • b* is the degree of yellowness, a high value being more yellow.
  • the results for batches 1 and 2 show that batch 2 is darker, with a lower L*. This is an indication of the degree of charring that occurred in the drier. The sample was noticeably darker when viewed by eye.
  • the protein cake still contained 5% dextrose on a dry solids basis.
  • the residence time of the wheat in the steep tank was 16 hours, the temperature was 48° C. and the water flow was 800 liters/hour.
  • the wheat exiting from the steep tank was first screened on a 1000 micron DSM screen to separate the wheat from water. It was then milled in mill which has a rotating toothed disc. The steep water was sent to waste
  • the milled wheat in a water slurry was then held in a small buffer tank.
  • the pH of the slurry was adjusted to pH 5.6 using caustic soda.
  • Amylase enzyme, Liquozyme Supra produced by Novozyme was added at a rate of 0.4 kg/hr at this point. It was pumped from this tank at a flow of 1.5 m 3 /hour to a jet cooker. This cooker was supplied with steam and the temperature of the mix was controlled at 110° C. After the jet cooker the mix was held for 5 minutes in a length of pipe to allow liquefaction of the starch to proceed before the pressure was released by passing through a valve allowing the mix to pass into a flash vessel at atmospheric pressure, where the temperature dropped to 98° C.
  • the slurry was then held in tanks for 3 hours at 98° C. to allow liquefaction to complete.
  • the pH was readjusted to pH 5.6 using sulphuric acid and a further 0.8 kg/hour of Liquozyme Supra was added. It was then pumped to a further flash vessel at 300 mbar where the temperature dropped to 62° C.
  • the pH was reduced to pH 4.2 and an amyloglucosidase enzyme, Dextrozyme DX supplied by Novozyme was added at a rate of 1.08 kg/hour.
  • the temperature of the contents was adjusted to between 28 and 30° C. and the contents stirred and allowed to ferment. Samples were taken at regular intervals and the ethanol and dextrose contents measured using HPLC. After 43.5 hours the contents of the flask were centrifuged. The solids component weighed 126.4 g. These solids were 15 dried overnight in a vacuum oven and the protein content measured at 66% protein on a dried solids basis.

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EP06752023A EP1880013A2 (fr) 2005-05-03 2006-05-02 Procede de concassage humide de cereales
AU2006242258A AU2006242258A1 (en) 2005-05-03 2006-05-02 Grain wet milling process for producing ethanol
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US11337442B2 (en) * 2014-11-14 2022-05-24 Roquette Freres Method for the valorisation of yeast biomass resulting from the production of ethanol
US11505838B2 (en) 2018-04-05 2022-11-22 Fluid Quip Technologies, Llc Method for producing a sugar stream
US11519013B2 (en) 2018-03-15 2022-12-06 Fluid Quip Technologies, Llc System and method for producing a sugar stream with front end oil separation
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